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Complexes of the Platinum Metals. Part 29. Pyridine-2-thiolate Derivatives of Ruthenium and Osmium: X-Ray Crystal Structures of and
Ruthenium and osmium precursors , , , , , and react with pyridine-2-thiol (pySH) or dipyridyl-2,2′-disulphide (pySSpy) in boiling benzene or toluene to afford a range of pyridin-2-thiolate complexes including , (2 isomers), , , and in which the pyridin-2-thiolate ligands are bound in monodentate (S-bonded) or bidentate (N,S-chelated) mode.Similar products are obtained from and in the presence of triethylamine and pyridine-2-thiol.The new complexes have been characterised by i.r. and n.m.r. (31P-<1H> and 1H) spectroscopy; reaction pathways are discussed.The X-ray crystal structures of and have been determined.The dicarbonyl , which undergoes facile conversion to , displays structural evidence of incipent attack by the non-co-ordinated N atom of the monodentate pyridine-2-thiolate ligand on a carbonyl group .Crystals of are monoclinic, space group P21/c, with a = 11.307(2), b = 11.083(3), c = 24.090(5) Angstroem, beta = 109.47(2) deg, and Z = 4.The structure, which has been refined to R = 0.045 for 4375 observed reflections, consists of highly distorted octahedral ruthenium(II) molecules with monodentate (S-bonded) and bidentate (N,S-bonded) pyridine-2-thiolate ligands, a cis pair of carbonyl groups, and a triphenylphosphine ligand trans to the S-bonded pyridin-2-thiolate.Crystals of are triclinic, space group P1, with a = 10.317(3), b = 11.749(3), c = 12.517(3) Angstroem, alpha = 67.65(2), beta = 70.55(2), gamma = 86.43(2) deg, and Z = 2.The structure, which has been refined to R = 0.040 for 12196 observed reflections consists of highly distorted octahedral ruthenium(II) molecules with a cis pair of bidentate (N,S-bonded) pyridine-2-thiolate ligands (trans S atoms), a carbonyl group, and a triphenylphosphine ligand.
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Reference£º
Highly efficient and robust molecular ruthenium catalysts for water oxidation,
Catalysts | Special Issue : Ruthenium Catalysts – MDPI